Bromotrimethylsilane → 1,5-Dibromo-2,3-dihydro-1H-indene
반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[CH:7](O)[CH2:6][CH2:5]2.[Br:12][Si](C)(C)C>C(Cl)(Cl)Cl>[Br:12][CH:7]1[C:8]2[C:4](=[CH:3][C:2]([Br:1])=[CH:10][CH:9]=2)[CH2:5][CH2:6]1참가 물질
4
실험 절차
To a nitrogen-purged flask was added 100 mg (0.469 mmol) of 5-bromoindan-1-ol from Step A and 3 mL of anhydrous chloroform, followed by 0.096 mL (0.704 mmol) of bromotrimethylsilane. The reaction mixture was stirred at ambient temperature overnight and concentrated. The residue was partitioned between ethyl acetate and water. The organic phase was washed with saturated aqueous sodium chloride solution, dried over sodium sulfate, and concentrated to give a brown oil which was used without further purification. Mass spectrum (MS): m/z 195, 197 (M+1-HBr), 116 (M+1-2HBr).
후처리
- customTo a nitrogen-purged flask
- concentrationconcentrated
- customThe residue was partitioned between ethyl acetate and water
- washThe organic phase was washed with saturated aqueous sodium chloride solution
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- customto give a brown oil which
- customwas used without further purification
출처 및 근거
- ORD 기록
- ord-ec62b51a66dc43eda88977270131fa42
- 출처 데이터셋
- uspto-grants-2007_07
- 특허 번호
- US07238683B2
반응 노트
불러오는 중…